CN108191927A - The removal methods of inorganic salts and organic impurities in a kind of Sucralose chloro liquid - Google Patents
The removal methods of inorganic salts and organic impurities in a kind of Sucralose chloro liquid Download PDFInfo
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- CN108191927A CN108191927A CN201810021023.9A CN201810021023A CN108191927A CN 108191927 A CN108191927 A CN 108191927A CN 201810021023 A CN201810021023 A CN 201810021023A CN 108191927 A CN108191927 A CN 108191927A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H13/00—Compounds containing saccharide radicals esterified by carbonic acid or derivatives thereof, or by organic acids, e.g. phosphonic acids
- C07H13/02—Compounds containing saccharide radicals esterified by carbonic acid or derivatives thereof, or by organic acids, e.g. phosphonic acids by carboxylic acids
- C07H13/04—Compounds containing saccharide radicals esterified by carbonic acid or derivatives thereof, or by organic acids, e.g. phosphonic acids by carboxylic acids having the esterifying carboxyl radicals attached to acyclic carbon atoms
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H1/00—Processes for the preparation of sugar derivatives
- C07H1/06—Separation; Purification
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Abstract
The invention discloses the removal methods of inorganic salts and organic impurities in a kind of Sucralose chloro liquid, 6 acetic acid esters of Sucralose in chloro liquid is directly extracted using organic solvent I, it is filtered the organic solvent containing 6 acetic acid esters of Sucralose is detached with inorganic salts, organic impurities after, filter residue adds organic solvent II and dissolves, washed filtering detaches organic impurities with inorganic salts；Organic impurities is converted into tractable carbon slag through carbonization treatment.It is distilled the invention avoids the waste water brought in extraction process as solvent using water and degradation problem, greatly reduces the difficulty and cost of wastewater treatment；And in system more than 98% inorganic salts can be separated, and chloro carbohydrate organic matter is not carried in the inorganic salts isolated secretly, avoid the problem of crystallization filtering is difficult caused by the enrichment of this type organic during Recycling Mother Solution is applied mechanically, also significantly reduce subsequent processing pressure simultaneously, the environmental protection treatment difficulty of waste residue degradation is effectively reduced, is suitble to industrialized production needs.
Description
Technical field
The present invention relates to chlorine in Chemical Manufacture Waste Disposal Technology field more particularly to a kind of sucrose trichloride production process
The method that inorganic salts and organic impurities are removed for liquid.
Background technology
Sucralose, abbreviation Sucralose is a kind of artificial synthesized high intensity sweetner, sugariness be sucrose 500~
It 600 times, because its is nontoxic, safety, being not involved in being metabolized in human body, not be absorbed by the body, sweet tea sense is also extremely similar to sucrose, because
This is by as a kind of ideal cane sugar substitution object.
Sucralose preparation process is using sucrose as raw material, by the way that the hydroxyl on specific 4,1 ', 6 ' position of sucrose is used
Chlorine atom replaces to obtain.The chlorinating agents such as generally use thionyl chloride carry out chlorination and prepare at high temperature in production process
Sucralose-6-acetic ester intermediate.Inevitably resulted from the reaction process chlorine, dichloro, tetrachloro, pentachloro- etc. other
Chloro impurity；Also, it needs to add in lye regulation system acid-base value after the completion of chloro, thus can also generate simultaneously a large amount of inorganic
Salt.Sucralose-6-acetic ester usually first from system is separated, then carried out at purification by current production technology
Reason further takes off ester and forms Sucralose.And sucralose-6-acetic ester is needed before purification process by inorganic salts
And other chloro impurity are separated in advance.
At present, the method for prior art removing inorganic salts and other chloro impurity mainly has following two：
When before DMF solvent is removed or after partial concentration DMF solvent, directly by filter method removing system
Inorganic salts.Whole operation is very high to seal and equipment the corrosion resistance requirement of filtration system, easily presss from both sides the inorganic salts of filtering
With high boiling solvent DMF, in this way, the inorganic salts filtered out remove DMF completely the methods of also needing to pass through drying, difficulty is very
Greatly.Also, it is dissolved in water and extracts after needing further solvent distillation due to the filtrate after filtering, thus can be by organochlorine for impurity
It is transferred in waste water, so as to increase microbial degradation difficulty.
Second is that after removing DMF solvent, it is directly added into a large amount of water and forms Aquo System, then extract by follow-up organic solvent
Inorganic salts, organochlorine are transferred to for impurity in water phase by step, and inorganic salt loading is precipitated by concentrating water phase, is separated by filtration,
Recycling Mother Solution is applied mechanically.But the method needs a large amount of water that could meet extraction process operation requirement, inevitably brings big
The waste water of amount improves the difficulty and operating cost of subsequent concentration distillation process.
Above two method all inevitably makes organochlorine in material be dissolved into water for impurity, and the COD of superelevation makes
It must degrade, decompose difficulty increasing.It can make its impurity enriched if recycled, solution becomes viscous, so as to hinder filtering point
From progress.If directly carrying out dangerous waste processing, because its water content is high, yield is big, processing cost is very high.
Invention content
It is an object of the invention to overcome the deficiencies of the prior art and provide inorganic salts in a kind of Sucralose chloro liquid and have
The removal methods of machine impurity are difficult effectively to reduce the difficulty of waste water distillation processing and cost and the environmental protection treatment of waste residue degradation
Degree.
The purpose of the present invention is achieved by the following technical programs：
The removal methods of inorganic salts and organic impurities in a kind of Sucralose chloro liquid provided by the invention, including following step
Suddenly：
(1) sucralose-6-acetic ester mixed solution is distilled by being concentrated under reduced pressure, and forms thick syrup；Then adding in has
Solvent I, stirring are precipitated crystal, obtain the mixed material after crystallization；
(2) mixed material after the crystallization is filtered, obtains I filtrate of black filter cake and organic solvent；It is described to have
I filtrate of solvent removes subsequent handling concentration purification sucralose-6-acetic ester；
(3) it after the filter cake is washed, adds in organic solvent II and is impregnated, filtered, obtain filter residue and organic solvent II
Filtrate；The filter residue is dissolved in water, filters out carbon slag therein, and obtains colourless or lurid inorganic salt solution；The nothing
The concentrated crystallization of machine salting liquid obtains inorganic salts and mother liquor, and the Recycling Mother Solution set is tied for the inorganic salt solution concentration of lower batch
Brilliant process；
(4) II filtrate of organic solvent obtains the organic underflow of brown through distillation and concentration, adds in the concentrated sulfuric acid and carries out at carbonization
Reason, the material after carbonization adds water to stir, and adds in lye and be neutralized to aqueous solution and be in neutrality, and is then filtered, obtain carbon slag and
Filtrate；The carbon slag merging treatment that the carbon slag is obtained with step (3), after the filtrate cycle set is used as lower batch stirring carbonization
Material use water.
The present invention directly extracts the sucralose-6-acetic ester in chloro liquid using organic solvent I, filtered to contain three
The organic solvent of chlorine cane sugar-6-acetic ester is detached for impurity (containing inorganic in the black filter cake filtered out with inorganic salts, organochlorine
Salt and highly polar organic impurities).Then, it will filter out the black filter cake come and washing filtering dissolved by organic solvent II, so as to
Organic impurities is detached with inorganic salts, organic impurities then by adding in concentrated sulfuric acid carbonization treatment, is converted into tractable carbon slag.
Further, the dosage of organic solvent I of the present invention is sucralose-6-acetic ester mixed liquor volume
100~300%.In the step (1), sucralose-6-acetic ester mixed solution is by concentration evaporator in 80~120 DEG C of temperature
Degree is lower to be concentrated under reduced pressure distillation；The organic solvent I adds at a temperature of 30~80 DEG C.
Further, in step (2) of the present invention, the mixed material after the crystallization is cooled to 10~30 DEG C and is taken out
Filter.
Further, in step (3) of the present invention, the filter cake is after organic solvent I washs and filters, washing filter
Liquid removes subsequent handling concentration purification sucralose-6-acetic ester with I filtrate of organic solvent.The dosage of the organic solvent II
10~50% for sucralose-6-acetic ester mixed liquor volume.
Further, in step (4) of the present invention, the dosage of the concentrated sulfuric acid is the 10~50% of organic underflow volume, excellent
It is selected as 20~30%.
Further, in step (4) of the present invention, 1~5h of stirring carbonization at a temperature of 80~100 DEG C, after carbonization
After material is cooled to 30~60 DEG C plus water stirs.
In said program, organic solvent I of the present invention is organic ester solvent, organic alcohol solvent, chloralkane；It is described to have
Machine ester solvent includes methyl acetate, ethyl acetate, butyl acetate；The organic alcohol solvent includes n-butanol, isobutanol；The chlorine
Include dichloromethane, chloroform, dichloroethanes, trichloroethanes for alkane.The organic solvent II is organic alcohol solvent, including
Methanol, ethyl alcohol, normal propyl alcohol, isopropanol.
The invention has the advantages that：
(1) present invention directly extracts the sucralose-6-acetic ester in chloro liquid using organic solvent, filtered to contain
The organic solvent of sucralose-6-acetic ester is detached with inorganic salts, organochlorine for impurity, and organic solvent used can pass through steaming
It evaporates recycling Posterior circle to use, be asked so as to avoid using water as the waste water distillation and degradation brought in extraction process after solvent
Topic greatly reduces the difficulty and cost of waste water distillation processing.
(2) present invention can separate more than 98% inorganic salts in system, and do not pressed from both sides in the inorganic salts isolated
Band chloro carbohydrate organic matter avoids crystallization caused by the enrichment of this type organic during Recycling Mother Solution is applied mechanically and filters difficult ask
Topic.In addition, by the concentrated sulfuric acid be carbonized chloro carbohydrate organic matter, make it into the COD value in microbiological treatment pond reduce 90% with
On, subsequent processing pressure is significantly reduced, the carbon slag after carbonization can carry out burning disposal as fuel, effectively reduce waste residue
The environmental protection treatment difficulty of degradation is suitble to industrialized production needs.
Below in conjunction with embodiment, the present invention is described in further detail.
Specific embodiment
After the embodiment of the present invention uses cane sugar-6-acetic ester by chlorination, lye and acid for adjusting pH value are added in, and take off
After solvent, the sucralose-6-acetic ester mixed solution that is formed.
Embodiment one：
The removal methods of inorganic salts and organic impurities in a kind of Sucralose chloro liquid of the present embodiment, its step are as follows：
(1) 500mL sucralose-6-acetic esters mixed solution is concentrated under reduced pressure by concentration evaporator at a temperature of 90 DEG C
Distillation forms thick syrup；Then 500mL ethyl acetate is added at a temperature of 30 DEG C, crystal is precipitated in stirring, after obtaining crystallization
Mixed material；
(2) mixed material after above-mentioned crystallization is cooled to room temperature to filter, obtains 47.5g black filter cake and 518ml
Ethyl acetate filtrate；After 30mL ethyl acetate washs and filters, washing filtrate merges subsequently filter cake with ethyl acetate filtrate
Process concentration purification sucralose-6-acetic ester；
(3) it is above-mentioned it is washed after filter cake, add in 100mL methanol and impregnate 30min, filter, obtain 35.8g filter residues and
105mL methanol filtrates；Filter residue adds in 20mL water dissolutions, filtering, obtains 15.3g carbon slag and the lurid inorganic salts of 33mL are molten
Liquid；The inorganic salt solution obtains 20.2g inorganic salts and 12mL mother liquors through independent condensing crystallizing, and Recycling Mother Solution set is for lower batch
Inorganic salt solution condensing crystallizing process；
(4) above-mentioned methanol filtrate obtains the organic underflow of 18mL brown through distillation and concentration, adds in the 5.4mL concentrated sulfuric acids, is warming up to
Stirring carbonization 5h at a temperature of 100 DEG C, the material after carbonization is cooled to 30 DEG C plus water stirring, and adds in wherein extra dense of alkali neutralization
Sulfuric acid to aqueous solution is in neutrality, and is then filtered, and obtains 10.7g carbon slag and 16mL filtrates；What the carbon slag was obtained with step (3)
Carbon slag carries out burning disposal or is handled as solid waste after merging, after filtrate cycle set is used as lower batch stirring carbonization
Material uses water.
Embodiment two：
The removal methods of inorganic salts and organic impurities in a kind of Sucralose chloro liquid of the present embodiment, its step are as follows：
(1) 500mL sucralose-6-acetic esters mixed solution is concentrated under reduced pressure by concentration evaporator at a temperature of 100 DEG C
Distillation forms thick syrup；Then 750mL methyl acetates are added at a temperature of 40 DEG C, crystal is precipitated in stirring, after obtaining crystallization
Mixed material；
(2) mixed material after above-mentioned crystallization is cooled to room temperature to filter, obtains 43.6g black filter cake and 756mL
Methyl acetate filtrate；After 50mL methyl acetates wash and filter, washing filtrate merges subsequently filter cake with methyl acetate filtrate
Process concentration purification sucralose-6-acetic ester；
(3) it is above-mentioned it is washed after filter cake, add in 150mL ethyl alcohol and impregnate 30min, filter, obtain 32.3g filter residues and
153mL ethanol filtrates；Filter residue adds in 20mL water dissolutions, filtering, obtains 12.9g carbon slag and the lurid inorganic salts of 31mL are molten
Liquid；The inorganic salt solution obtains 17.7g inorganic salts and 10mL mother liquors through independent condensing crystallizing, and Recycling Mother Solution set is for lower batch
Inorganic salt solution condensing crystallizing process；
(4) above-mentioned ethanol filtrate obtains the organic underflow of 17mL brown through distillation and concentration, adds in the 3.4mL concentrated sulfuric acids, is warming up to
Stirring carbonization 5h at a temperature of 100 DEG C, the material after carbonization is cooled to 40 DEG C plus water stirring, and adds in wherein extra dense of alkali neutralization
Sulfuric acid to aqueous solution is in neutrality, and is then filtered, and obtains 9.5g carbon slag and 15mL filtrates；What the carbon slag was obtained with step (3)
Carbon slag carries out burning disposal or is handled as solid waste after merging, after filtrate cycle set is used as lower batch stirring carbonization
Material uses water.
Embodiment three：
The removal methods of inorganic salts and organic impurities in a kind of Sucralose chloro liquid of the present embodiment, its step are as follows：
(1) 500mL sucralose-6-acetic esters mixed solution is concentrated under reduced pressure by concentration evaporator at a temperature of 100 DEG C
Distillation forms thick syrup；Then 1000mL butyl acetates are added at a temperature of 30 DEG C, crystal is precipitated in stirring, after obtaining crystallization
Mixed material；
(2) mixed material after above-mentioned crystallization is cooled to room temperature to filter, obtains 45.1g black filter cake and 1008mL
Butyl acetate filtrate；After 50mL butyl acetates wash and filter, washing filtrate merges subsequently filter cake with butyl acetate filtrate
Process concentration purification sucralose-6-acetic ester；
(3) it is above-mentioned it is washed after filter cake, add in 150mL normal propyl alcohols and impregnate 30min, filter, obtain 34.5g filter residues and
152mL normal propyl alcohol filtrates；Filter residue adds in 20mL water dissolutions, filtering, obtains 13.6g carbon slag and the lurid inorganic salts of 33mL
Solution；The inorganic salt solution obtains 18.8g inorganic salts and 12mL mother liquors through independent condensing crystallizing, and Recycling Mother Solution set is for lower batch
Secondary inorganic salt solution condensing crystallizing process；
(4) above-mentioned normal propyl alcohol filtrate obtains the organic underflow of 17mL brown through distillation and concentration, adds in the 1.7mL concentrated sulfuric acids, heating
Stirring carbonization 5h at a temperature of to 100 DEG C, the material after carbonization is cooled to 40 DEG C plus water stirring, and it is wherein extra to add in alkali neutralization
The concentrated sulfuric acid to aqueous solution is in neutrality, and is then filtered, and obtains 10.9g carbon slag and 12mL filtrates；The carbon slag is obtained with step (3)
Carbon slag merge after carry out burning disposal or handled as solid waste, after filtrate cycle set is used as the stirring carbonization of lower batch
Material use water.
Claims (10)
1. the removal methods of inorganic salts and organic impurities in a kind of Sucralose chloro liquid, it is characterised in that include the following steps：
(1) sucralose-6-acetic ester mixed solution is distilled by being concentrated under reduced pressure, and forms thick syrup；Then it adds in organic molten
Agent I, stirring are precipitated crystal, obtain the mixed material after crystallization；
(2) mixed material after the crystallization is filtered, obtains I filtrate of black filter cake and organic solvent；It is described organic molten
I filtrate of agent removes subsequent handling concentration purification sucralose-6-acetic ester；
(3) it after the filter cake is washed, adds in organic solvent II and is impregnated, filtered, obtain II filtrate of filter residue and organic solvent；
The filter residue is dissolved in water, filters out carbon slag therein, and obtains colourless or lurid inorganic salt solution；The inorganic salts are molten
The concentrated crystallization of liquid obtains inorganic salts and mother liquor, and the Recycling Mother Solution set is used for the inorganic salt solution condensing crystallizing work of lower batch
Sequence；
(4) II filtrate of organic solvent obtains the organic underflow of brown through distillation and concentration, adds in the concentrated sulfuric acid and carries out carbonization treatment, carbon
Material after change adds water to stir, and adds in lye and be neutralized to aqueous solution and be in neutrality, and is then filtered, obtains carbon slag and filtrate；
The carbon slag merging treatment that the carbon slag is obtained with step (3), the filtrate cycle set are used as the object after lower batch stirring carbonization
Material uses water.
2. the removal methods of inorganic salts and organic impurities in Sucralose chloro liquid according to claim 1, feature exist
In：The dosage of the organic solvent I is the 100~300% of sucralose-6-acetic ester mixed liquor volume.
3. the removal methods of inorganic salts and organic impurities in Sucralose chloro liquid according to claim 1, feature exist
In：In the step (1), sucralose-6-acetic ester mixed solution is depressurized by concentration evaporator at a temperature of 80~120 DEG C
Concentration distillation；The organic solvent I adds at a temperature of 30~80 DEG C.
4. the removal methods of inorganic salts and organic impurities in Sucralose chloro liquid according to claim 1, feature exist
In：In the step (2), the mixed material after the crystallization is cooled to 10~30 DEG C and is filtered.
5. the removal methods of inorganic salts and organic impurities in Sucralose chloro liquid according to claim 1, feature exist
In：In the step (3), the filter cake is after organic solvent I washs and filters, washing filtrate and I filtrate of organic solvent
Remove subsequent handling concentration purification sucralose-6-acetic ester.
6. the removal methods of inorganic salts and organic impurities in Sucralose chloro liquid according to claim 1, feature exist
In：The dosage of the organic solvent II is the 10~50% of sucralose-6-acetic ester mixed liquor volume.
7. the removal methods of inorganic salts and organic impurities in Sucralose chloro liquid according to claim 1, feature exist
In：In the step (4), the dosage of the concentrated sulfuric acid is the 10~50% of organic underflow volume.
8. the removal methods of inorganic salts and organic impurities in Sucralose chloro liquid according to claim 7, feature exist
In：In the step (4), the dosage of the concentrated sulfuric acid is the 20~30% of organic underflow volume.
9. the removal methods of inorganic salts and organic impurities in Sucralose chloro liquid according to claim 1, feature exist
In：In the step (4), 1~5h of stirring carbonization at a temperature of 80~100 DEG C, after the material after carbonization is cooled to 30~60 DEG C
Water is added to stir.
10. the removal methods of inorganic salts and organic impurities in Sucralose chloro liquid according to claim 1, feature exist
In：The organic solvent I is organic ester solvent, organic alcohol solvent, chloralkane；Organic ester solvent include methyl acetate,
Ethyl acetate, butyl acetate；The organic alcohol solvent includes n-butanol, isobutanol；The chloralkane includes dichloromethane, three
Chloromethanes, dichloroethanes, trichloroethanes.The organic solvent II is organic alcohol solvent, including methanol, ethyl alcohol, normal propyl alcohol, isopropyl
Alcohol.
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| CN201810021023.9A CN108191927B (en) | 2018-01-10 | 2018-01-10 | Method for removing inorganic salt and organic impurities in sucralose chloride solution |
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| CN201810021023.9A CN108191927B (en) | 2018-01-10 | 2018-01-10 | Method for removing inorganic salt and organic impurities in sucralose chloride solution |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109678912A (en) * | 2018-12-10 | 2019-04-26 | 安徽金禾实业股份有限公司 | A kind of processing method of Sucralose neutralizer concentrated residue |
| CN109734755A (en) * | 2018-12-28 | 2019-05-10 | 山东三和维信生物科技有限公司 | A kind of Sucralose crystallization processes |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102321122A (en) * | 2011-10-21 | 2012-01-18 | 湖北益泰药业有限公司 | Method for preparing sucralose from sucralose-6-acetate |
| CN106674292A (en) * | 2016-12-09 | 2017-05-17 | 福建科宏生物工程股份有限公司 | Method for purification treatment of sucralose water crystallization mother liquor |
| CN106674293A (en) * | 2016-12-09 | 2017-05-17 | 福建科宏生物工程股份有限公司 | Method for treating sucralose-6-acetic acid ester waste mother liquor in hydrolysis mode |
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2018
- 2018-01-10 CN CN201810021023.9A patent/CN108191927B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102321122A (en) * | 2011-10-21 | 2012-01-18 | 湖北益泰药业有限公司 | Method for preparing sucralose from sucralose-6-acetate |
| CN106674292A (en) * | 2016-12-09 | 2017-05-17 | 福建科宏生物工程股份有限公司 | Method for purification treatment of sucralose water crystallization mother liquor |
| CN106674293A (en) * | 2016-12-09 | 2017-05-17 | 福建科宏生物工程股份有限公司 | Method for treating sucralose-6-acetic acid ester waste mother liquor in hydrolysis mode |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109678912A (en) * | 2018-12-10 | 2019-04-26 | 安徽金禾实业股份有限公司 | A kind of processing method of Sucralose neutralizer concentrated residue |
| CN109678912B (en) * | 2018-12-10 | 2022-03-04 | 安徽金禾实业股份有限公司 | Method for treating concentrated residue of sucralose neutralized solution |
| CN109734755A (en) * | 2018-12-28 | 2019-05-10 | 山东三和维信生物科技有限公司 | A kind of Sucralose crystallization processes |
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